Distillation apparatus



DISTILLATION APPARATUS Filed July 14, 1932 Patented Jan. 1935 WilliamSieck, Jr., Hubbard Woods, m, assignor to William Gan'ique & Company,Inc., Chicago,- IlL, a corporation of Illinois Application July 14,1932, Serial No. 622,484

4 Claims.

A further object is to provide in an apparatus.

of this character a reflux column for the separation of the vapors, andwhich column is provided with means for regulating the temperature ofthe column, a condenserwith which the column is connected to eifectcomplete or partial condensa tion of the vapors leaving the column, anda steam ejector for maintaining a high vacuum in the entire system.

To the attainment of these ends and the accomplishment of other new anduseful objects as will appear, the invention consists in the features ofnovelty in substantially the construction, 25 combination andarrangement of the several parts hereinafter more fully described andclaimed and shown in the accompanying drawing illustrating thisinvention, and in which I The figure is a diagrammatic cross-sectionalview of an apparatus of this character constructed in accordance withthe principles of this invention. a

, Referring more particularly to the drawing, the

3 numeral 1 designates generally a still of any suitable material,fitted with a heating coil 2 into which latter steam, or a heatingfluid, may be cessive resistance.

admitted through a valve 3 and, discharged through an outlet 4.

40 a discharge valve 6 for. removing the residue of the distillation,and is also provided with a perforated pipe 7 or a number of perforatedpipes therein and near the bottom thereof, for the purpose of admittingsteam directly into the mate-' rial to be distilled. The top of thestill is fitted with a vapor outlet 8 which has communication with andextends to a separator 9. Theseparator preferably consists of a shellwith a tangential inlet opening 8 through which thevapors from the still1 are admitted.

Extending into the separator is an outlet pipe 10 which is preferablyflared out at the lower end, and is covered at the lower end with a finemesh screen or perforated metal disc 9 The still is provided with afllling valve 5 and A drain pipe 11 leads from the bottom of theseparator 9 to the still 1 and enters thestill, terminating at a pointbelow the normal liquid level 48 in the still.

' The outlet pipe 10 which leads from the top of the separatorcommunicates with aheat interchanger 12, preferably of a tubular 'typ'e,consisting of a casing 13 provided with tube sheets 14, into whichlatter are extended the ends of the tubes 15. The ends of these tubesopen into two end compartments 69-70 arranged in the v heat interchangerso'that steam admitted through the opening19 into the compartment70'will flow through the tubes 14 into the other compartment 69 and willpass out through-an opening 26. a

' The bottom of the'casing 13 is provided with a vapor outlet 16 whichis connected to a reflux column 18 by means of a pipe 17. The outlet 19I is connected to a desuperheater 21 by means of a pipe 20. The opening26 of the heat interchanger 12 is provided with a pipe 27 leadingtherefrom a and communicating with the perforated pipe .7v

in the still. v Y The desuperheater 21 preferably consists 01. a closedtank with a perforated metal plate 22,,upon which latter is preferablyplaced suitable packing material 23, to constitute. extended surfacesfor thedeposit of condensation and between which material the vapors andgases pass without ex- Steam enters the desuper-' heater through aninlet valve 24-and water en ters through a valve 25.

The column 18 is provided with a discharge "valve 28 to remove thefinished product, and a heating coil 29 to which steam, or a heatingfluid, may be admitted through a valve 30 and dis- 1 charged through anoutlet 31.

The lower column tray 32 has in its centeria vapor opening 33 providedwith an encompassing vertical rim or flange, and'with a drain pipe34,.which latter extends toward and termi-' nates adjacent the bottom ofthe column. Perforated plates 35 are providedjand thereuponis placedsuitable packing material 36, between which the vapors may pass. isprovided with a vapor opening 38 encompassed by a vertical rim, and thecolumn itself A-column tray 3'1 has adjac'ent'the tray an opening 39 towhich is connected apipe 44 which has communicationwith a closed tank42-. The pipe 44 is preferably provided with a valve 40, the opening ofwhich valve allows theliquid in the tray to' drain into the tank 42. Theliquid is removed from the tank 42 by means of a drain valve 43, and

a vacuum breaking valve 41. The numeral 45 represents a pipe forsupplying water or any other liquid to the column, the supply of whichis controlled by means of :avalve 46.

In order to obtain a good distribution of this water over the entirecross section of the column, the end of the pipe 45 is preferably fittedwith a spray nozzle of any suitable construction.

Leading from the column 18 is a vapor outlet which has communicationwith a condenser 49,

- by means of 'a pipe 47. The condenser 49 is preferably of a tubulartype consisting of a casing 51 provided with tube sheets through whichare extended the ends of the tube 50, and through which latter thecooling medium flows, the vapors to be condensed passing around theoutside thereof. The condenser is provided with a discharge valve 52connected to a pipe 53,- which latter communicates with and extends, toa closed tank 54. The opening of the valve 52 allows condensates fromthe condenser 49 to flow into the tank 54 and are removed from thelatter by means of a valve 55, and a vacuum breaker valve 56 may beprovided.

The condenser 49 is connected to an ejector 60, preferably of the jettype, consisting of a throat member 58 and a steam nozzle 68, the flowof steam to the latter being controlled by a valve The discharge end ofthe ejector is connected to a condenser 64 preferably of the barometrictype, consisting of a condensing chamber 62 and a barometric leg 65,terminating in a hot well 66. The condenser 64 is provided with a watersupply pipe 63, and an outlet 61 leading from the condensing chamber andthrough which cut-- by means of the points of water ine vapors will letpipe air or other non-condensable gases may be removed by means of avacuum pump (not shown) or any other suitable means. A description ofthe operation of the apparatus will be given in the distillationofglycerine, but

it is to be understood that it is not desired to.

be limited to this particular product, as other products may bedistilled in the apparatus with equal efiiciency. The still 1 is filledto a level approximately indicated at 48, with crude glycerine, andsteam is admitted to the coil 2. The steam ejector 60' is then set intooperation, and the whole system is exhausted thereby to a vacuumof atleast twenty-nine inches of mercury.

The steam valve 24 is gradually opened to admit steam into thedesuperheater 21. Water is then admitted through the spray pipe by meansof the valve 25, until the temperature of the steam leaving thedesuperheater is that corresponding to a vacuum of about twenty totwenty-flve inches of mercury; Water will be evaporated or flashed intosteam and this will withdraw enough heat from the live steam to reduceits temperature. The desuperheated steam flowsthrough the tubes of theheat interchanger 12 and finally through the'glycerine in the stillpipes 27-7. The mixture of hot glycerine vapor and steam will passupthrough the outlet pipe sand into the separator 9. Any

entrained liquids in the separator will be thrown or forced into thebottom of the separator and will drain or flow back into the still 1through, the pipe 11, and the r the pipe 10 to the heat interchanger 12.

vapors will proceed through Due to the large diilerence in the boilingand glycerine, someof the glycerbe condensed in the heat interchanger12, and will now in the form of a liquid,

1'7, together with the remaining vapors now containing a higherpercentage of steam. By maintaining the proper temperature in the steamflowing through the tubes of the heat interchanger, the glycerinecondensed at this point will be of high gravity and high purity.

At the same time the latent heat of condensation of the glycerinecondensed in the heat interchanger 12 will be transferred to thedesuperheated steam flowing through the tubes 15, resulting, in thesuperheating of the steam leaving the heat interchanger and entering theglycerine in the still 1' through the pipes 27 and perforated pipe '7. 5

The uncondensed glycerine vapors and steam pass up through theperforated plates 3735 and pervious pack-' ing material thereupon. Dueto the reflux action of the plates and the pervious packing materialeach plate will accumulate a mixture of glycerine and water, and-theconcentration of the glycerine in this mixture will vary on thedifferent plates, being high on the lower plates and low on the upperplates, in fact if temperature and vacuum the reflux column 18 through.

conditions are properlyf controlled the upper plates will containpractically pure water.

Due to condensation of glycerine on the plates 35 37, and-on thepervious material, heat will be liberted, and unless this liberated heatis controlled, the temperature of the vapors and liquid in the columnwill rise, allowing glycerine vapors to reach the top of the column Toprevent this, water is injected into the column by meansof the spray.water, upon flashing into steam, .will absorb heat and tend to cool thevapors passing to the'upper plates.

Vapor composition curves oi'- glycerine and water mixtures boiling undera high vacuum show the glycerine content of these. vapors to pipe 45,and which injected C. The introduction of water from, the spray and .itsevaporation will tend to establish this condition on the upper platesand prevent loss of glycerine from the top of the column.

The water vapors and non-condensable gases leaving the column 18 passthrough the tubular condenser 49 where condensed, depending on thetemperature of the. cooling medium. I

The remaining water vapor and non-condensable gases will be removed bythe ejector 60 to and the steam admitted to the elector will becondensed, and from which, the non-condensable gases are removed throughthe pipe 61 by means of ejectors or vacuum pumps (not shown).

The liquid dripping from the bottom plate 35 on to the tray 32 will berich in-glycerine and will flow to the bottom section of the columnthroughthe pipe 34. Steam is admitted to the 001129, and theconcentrated glycerine from the column and the interchanger is heated toboil oi! some of the water may be the condenser .62 in which latter thewater vapors I the remaining water until proper concentration isreached. Any low boiling fractions will gradually collect on the tray37, and will, from time to time, be drained to the pipe 44.

While the preferred method and apparatus for carrying this inventionherein described, itis to ous changes may be in the steps of the methodof into operationhave been be understood that variprocess, withinthethetankflbymeansofmad e in thdapparatus and scope of the claims, withoutdeparting from the spirit of this invention.

What is claimed as new is:

1. A distilling apparatus embodying a still, a separator for receivingand separating from the vapors from the still foreign particles andentrained liquid in the vapors, a heat interchanger with which theseparator is connected,

means for circulating a cooling fluid through the heat interchanger outof commingling relation with the vapors therein, the temperature of thecooling fluid being raised thereby, means for discharging the heatedcooling fluid into the still, a reflux column, means for discharging thecondensed and uncondensed vapors from the heat interchanger into thesaid reflux column, and means for discharging a cooling liquid into thesaid reflux column in commingling relation with the fluid therein toextract the remaining degree of heat by reducing the temperaturecausedby the condensation of the vapors.

2. A distilling apparatus embodying a still, a separator for receivingand separating from the vapors from the still foreign particles andentrained liquids in the vapors, a heat interchanger with which theseparator is connected. means for circulating a cooling fluid throughthe heat interchanger out of 'commingling relation with the vaporstherein, the temperature of the cooling fluid being raised thereby,means for discharging the heated cooling fluid into the still, a refluxcolumn, means for discharging the condensed and uncondensed vapors fromth; heat interchanger into the said reflux column, means for discharginga cooling liquid into the said reflux column in commingling relationwith the fluid therein to extract remaining degree of heat by reducingthe temperature caused by the condensation of the vapors, a condenser,means for passing vapors from the top of the reflux column into thecondenser, and means for drawing any remaining vapors from saidcondenser.

3. A distilling apparatus embodying a still, 'a separator for receivingvapors from the still and for separating foreign particles and entrainedliquid therefrom, a heat interchanger for receiv ing vapors from theseparator, a reflux column for receiving condensed and uncondensedvapors from the heat interchanger, said heat interchanger embodyingspaced chambers, passages forming communication between said chambersand constituting condensation surfaces, means forming communicationbetween one of said chambers and said still, an additional chambercommunicating with the other chamber in the heat interchanger, means foradmitting liquid into the said additional chamber, and means foradmitting aheating medium into the said additional chamber to flash thelast said liquid into steam to be circulated through said heatinterchanger and into the still.

.4. A distilling apparatus embodying a still, a separator for receivingvapors from the still and for separating foreign particles and entrainedliquid therefrom, a heat interchanger for receiving vapors from theseparator, a reflux column for receiving condensed and uncondensedvapors from the heat interchanger, said heat interchanger embodyingspaced chambers, passages forming communication between said chambersand constituting condensation surfaces, means forming communicationbetween one of said chambers and said still, an additional chambercommunicating with the other chamber in the heat interchanger, means foradmitting liquid into the said additional chamber, means for admitting aheating medium into the said additional chamber to flash the last saidliquid into steam to be circulatedthrough said heat interchanger andinto the still, and means individual to the last said liquid supplyingmeans and the said heating medium for controlling them.

WILLIAM SIECK, JR.

CERTIFICATE OF CORRECTION.

Patent No. 1,986,165." .7 Januaryl. 1935.

4 mumsmcx, JR.

It is hereby certified that the name of the assignee in the abovenumbered patent was erroneously writtenand printed as "William Garrique& Company, Inc. whereas said name should have been written and printedas WilliamGarrigue 8: Company, Inc. as shown by the records ofassignments in this office; and that the said Letters Patent should beread with this correction therein that the same may conform to therecord of the case in the Patent Office. v

Signed and sealed this 19th day of February, A. I). 1935.

, I Leslie Frazer (Seal) Acting Commissioner of Patents.

